CN104927762A - Worm-bore-like porous-carbon/magnetic particle compound absorbent and preparation method thereof - Google Patents
Worm-bore-like porous-carbon/magnetic particle compound absorbent and preparation method thereof Download PDFInfo
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- CN104927762A CN104927762A CN201510292093.4A CN201510292093A CN104927762A CN 104927762 A CN104927762 A CN 104927762A CN 201510292093 A CN201510292093 A CN 201510292093A CN 104927762 A CN104927762 A CN 104927762A
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Abstract
A worm-bore-like porous-carbon/magnetic particle compound absorbent and a preparation method thereof belong to the technical field of electromagnetic wave absorption materials. Polyacrylonitrile and Co-doped ferriferrous oxide particles coated with silica are mixed according to a certain proportion in a solution mixing manner to obtain a polyacrylonitrile/magnetic particle solution; a glass plate is coated with the solution, the coated glass plate is quickly moved into water, soaked and then taken out to be dried in air to obtain a polyacrylonitrile/magnetic particle porous composite film; the obtained polyacrylonitrile/magnetic particle porous composite film is pre-oxidized and carbonized at a certain temperature, and the pre-oxidized and carbonized polyacrylonitrile/magnetic particle porous composite film is ground to obtain the worm-bore-like porous-carbon/magnetic particle compound absorbent, wherein the mass ratio of porous carbon and the magnetic particles is (75-85): (25-15), and the diameter of the worm-bore-like holes is 40-100 nm. The prepared graphitized multi-wall carbon nano-tube/nano-particle compound absorbent further takes paraffin as the matrix, and wave-absorbing materials with different absorbent filling volumes can be prepared.
Description
Technical field
The invention belongs to electromagnetic wave absorbent material technical field, particularly relate to kind worm hole porous carbon/magnetic particle composite wave-absorbing agent and preparation method thereof.
Background technology
In recent years, along with the fast development of electronic industry, electromagnetic pollution is on the rise, and absorbing material serves vital effect in electromagnetic pollution protection field.Simultaneously realize military equipment radar invisible, weaken electromagnetic interference, the field such as ensure information security, absorbing material has also played very important effect.Absorbing material (microwave absorbing material, electromagnetic wave attenuation material or Radar Stealth Materials) can reduce the reflection of hertzian wave at body surface effectively, makes the hertzian wave inciding material internal be efficiently damped simultaneously.Absorbing material can be divided into wave absorbing agent and matrix according to its composition.Matrix mainly plays the effect of bonding in absorbing material, and wave absorbing agent is the main body of absorbing material, plays the effect of hertzian wave loss.The demand of outstanding wave absorbing agent demand fulfillment lightweight, the aspect such as absorption intensity is large, absorption band is wide, electromagnetic consumable ability is strong and environmental resistance is strong.
Carbon material, has the advantage of the aspects such as good chemical stability, excellent thermostability, high physical strength and outstanding conductivity.The quality of carbon material is light simultaneously, has larger potentiality in the outstanding wave absorbing agent field of preparation.But, according to transmission line theory (Qin, F.; Brosseau, C., J.Appl.Phys.2012,111,061301), for the wave absorbing agent (dielectric loss type or magnetic loss type) of one-component, owing to being difficult to the coupling realizing good electromagnetic parameter in same material, so the final absorbing property of material is limited, gradually can not meet that absorbing material is efficient, the requirement of lightweight and wideband, therefore preparation has the composite wave-absorbing agent of dielectric loss and magnetic loss concurrently, two kinds of losses is effectively combined, has become the focus of current absorbing material research field.Composite wave-absorbing agent has electromagnetic matching ability relatively preferably, effectively can reduce the reflection of hertzian wave on absorbing material surface, hertzian wave is made can effectively to enter absorbing material inside, by dielectric loss and the magnetic loss of material, hertzian wave is absorbed effectively, obtain excellent absorbing property, play more and more important role in absorbing material field.But the introducing of magneticsubstance, often make the wave absorbing agent prepared have larger density, this is disadvantageous for the quality alleviating absorbing material.So, the focus be designed in order to nowadays lightweight absorbing material research field of porous absorbing material.Meanwhile, the introducing of vesicular structure, can increase the contact probability of hertzian wave and wave absorbing agent effectively, and the interaction of hertzian wave and wave absorbing agent is increased, hertzian wave fast and effeciently loss that can be the most incident.Therefore, the agent of porous composite wave-absorbing plays more and more important role in absorbing material field.
Summary of the invention
Class worm hole porous carbon/magnetic particle composite wave-absorbing agent that the invention provides a kind of absorbing property excellence and preparation method thereof.The preparation technology of this composite wave-absorbing agent is simple, convenient operation, is easy to produce, the material simultaneously prepared has vesicular structure, and its absorbing property is excellent, has wider suction ripple frequency band, stronger absorption intensity, the characteristics such as lightweight, have larger application potential in absorbing material field.In the present invention, take polyacrylonitrile as matrix, by the method for the magnetic particle of coated with silica by solution blending, mix in polyacrylonitrile, prepare porous polypropylene nitrile/magnetic particle composite membrane by the method for inversion of phases, the composite membrane obtained is obtained through preoxidation, carbonization and grinding there is class worm hole porous carbon/magnetic particle composite wave-absorbing agent.The wave absorbing agent absorbing property of preparation is excellent, shows for electromagnetic C-band (4 ~ 8GHz), X-band (8 ~ 12GHz) and K
uthe absorption that wave band (12 ~ 18GHz) is stronger, its maximum reflection loss reaches-36dB (Fig. 6 can reflect).
Class worm hole porous carbon/magnetic particle composite wave-absorbing agent provided by the present invention, the mass ratio of porous carbon and magnetic particle is 75 ~ 85:25 ~ 15, the diameter of class worm hole is 40 ~ 100nm (this some holes is all through hole, is also to be communicated with between hole and hole).
The preparation process of composite wave-absorbing agent is divided into following three steps: mixed according to the mode of certain ratio by solution blending with the cobalt doped Z 250 particle of coated with silica by polyacrylonitrile, obtain polyacrylonitrile/magnetic particle solution; Be coated on by solution on sheet glass, fast transfer, in water, soaks, obtains polyacrylonitrile/magnetic particle porous composite film after taking-up in air drying; By obtain polyacrylonitrile/magnetic particle porous composite film preoxidation at a certain temperature, carbonization, grinding obtain that there is class worm hole porous carbon/magnetic particle composite wave-absorbing agent.
The preparation method of class worm hole porous carbon/magnetic particle composite wave-absorbing agent of the present invention, its concrete step is as follows:
(1) under nitrogen protection, to in 150 ~ 250mL distilled water, add 5 ~ 6mmol ferric chloride hexahydrate, 2.0 ~ 2.5mmol Iron dichloride tetrahydrate and 0.4 ~ 0.6mmol cobalt chloride hexahydrate, it is 9 ~ 11 to pH that warming-in-water to 60 ~ 80 DEG C add strong aqua (mass percent 25 ~ 28%) wherein, continue reaction 30 ~ 90min, Magneto separate reclaims, and uses distilled water and dehydrated alcohol respectively to wash 5 ~ 8 times recovery product, is scattered in 5 ~ 15mL distilled water; Dispersion liquid is joined in 200 ~ 400mL ethanol, at 30 ~ 50 DEG C, add 5 ~ 7mL distilled water, 7 ~ 9mL strong aqua (mass percent 25 ~ 28%), 0.8 ~ 1.2mL tetraethyl orthosilicate, reaction 9 ~ 11h; Magneto separate reclaims, and uses distilled water and dehydrated alcohol respectively to wash 5 ~ 8 times recovery product, is then placed in vacuum drying oven 60 ~ 90 DEG C of drying 10 ~ 15h, obtains the cobalt doped Z 250 particle of coated with silica;
(2) the cobalt doped Z 250 particle of 0.25 ~ 0.40g coated with silica is used 12 ~ 16mL dimethyl formamide (DMF, also can be N,N-DIMETHYLACETAMIDE, because the polyacrylonitrile used below only in strong solvent solvability better) ultrasonic disperse 1 ~ 3h, add 2.0 ~ 3.0g polyacrylonitrile, 0.1 ~ 0.2g Polyvinylpyrolidone (PVP), 50 ~ 70 DEG C of heating for dissolving 1 ~ 3h, solution is poured on the flat board of surfacing, in distilled water, 12 ~ 36h is soaked after knifing, air drying 12 ~ 36h after taking out, obtain polyacrylonitrile/magnetic particle porous composite film,
(3) by polyacrylonitrile/magnetic particle porous composite film heat treated 3 ~ 6h at 200 ~ 300 DEG C of preparation, and then under 900 ~ 1100 DEG C of vacuum carbonizing treatment 0.5 ~ 2h, obtain porous carbon/magnetic particle composite membrane, composite membrane is fully ground, obtains class worm hole porous carbon/magnetic particle composite wave-absorbing agent.
Greying multi-walled carbon nano-tubes/Nanocomposites the wave absorbing agent utilizing the present invention to prepare, take paraffin as matrix further, can prepare the absorbing material of different wave absorbing agent loading level, its method prepared is as follows:
(1) by paraffin and class worm hole porous carbon/magnetic particle composite wave-absorbing agent mixing, in mixture, the mass percentage of wave absorbing agent is 25% ~ 35%;
(2) mixture step (1) obtained uses oil press to be suppressed into the test annulus that external diameter is 7mm, internal diameter is 3mm by mould; Thickness 2mm;
(3) use Agilent N5244A PNA-X test the electromagnetic parameter of above-mentioned obtained sample within the scope of 2 ~ 18GHz (ε ', ε ", μ '; μ "), utilize reflection loss RL (Lu Shaowei, the Li Qian of this composite wave-absorbing agent of following formulae discovery, bear needs sea, mark is bright, Xu Weikai, Jia Caixia, Journal of Inorganic Materials, 2015,30,23-28).
In formula: Z
0that free space impedance (passes through μ
0, ε
0use formulae discovery); μ
0, ε
0permeability of vacuum and specific inductivity, ε
0=8.854187817 × 10
-12f/m, μ
0=4 π × 10
-7h/m; Z
inbe absorbing material input resistance (utilize ε ', ε ", μ ', μ " data calculation); F is electromagnetic frequency (scope is 2 ~ 18GHz); D is the thickness of absorbing material; C is the velocity of propagation of hertzian wave at freeboard, equals the light velocity 3 × 10
8m/s; ε
r(ε
r=ε '-j ε ") and μ
r(μ
r=μ '-j μ ") be the relative complex dielectric permittivity of equivalence and the complex permeability of absorbing material, j is the imaginary part unit of complex dielectric permittivity and complex permeability, without practical significance.Experiment can record the ε ' of material under different wave frequency f, ε ", μ ', μ ".
Accompanying drawing explanation
Fig. 1: the cobalt doped Z 250 particle of coated with silica prepared by embodiment 1 and embodiment 2 and class worm hole porous carbon/magnetic particle composite wave-absorbing agent XRD spectra.
Fig. 2: the stereoscan photograph of porous carbon/magnetic particle composite membrane prepared by embodiment 2, illustration is composite membrane partial enlarged drawing.
Fig. 3: the stereoscan photograph of class worm hole porous carbon/magnetic particle composite wave-absorbing agent prepared by embodiment 2, illustration is composite wave-absorbing agent partial enlargement electromicroscopic photograph.
Fig. 4: the hole diameter distribution plan of the class worm hole porous carbon/magnetic particle composite wave-absorbing agent of preparation in embodiment 2.
Fig. 5: the energy spectrum analysis data plot of class worm hole porous carbon/magnetic particle composite wave-absorbing agent prepared by embodiment 2.
Fig. 6: the reflection loss RL data plot that the electromagnetic parameters of the class worm hole porous carbon/magnetic particle composite wave-absorbing agent utilizing embodiment 3 to test obtains.
Fig. 1 gives the Z 250 particle of the cobalt doped of the coated with silica of preparation and the XRD spectra of class worm hole porous carbon/magnetic particle composite wave-absorbing agent, analysis of spectra is known, the purity of the cobalt doped Z 250 particle of the coated with silica of preparation is higher, and carbon degree of crystallinity is relatively little in the class worm hole porous carbon/magnetic particle composite wave-absorbing agent obtained, this unformed structure can bring active influence for the polarization in the electric field of material, and the diffraction peak of the Z 250 of cobalt doped disappears substantially, what occur is the diffraction peak of iron and cobalt nanometer particle, illustrate that the Z 250 of cobalt doped is at high temperature reduced to cobalt simple substance and iron simple substance, and this change also can bring certain impact to the absorbing property that material is final.
The photo of the scanning electron microscope of the porous carbon/magnetic particle composite membrane of preparation that what Fig. 2 provided is, as can be seen from the photo of scanning electron microscope, the composite membrane obtained has obvious finger hole structure, and its cell walls then shows as the nano pore structure with class worm pore space structure.
What Fig. 3 provided is through grinding the stereoscan photograph of the composite wave-absorbing agent obtained in embodiment 2, found by electromicroscopic photograph, through grinding, finger hole destroys, and the nanoporous with class worm pore space structure on duct obtains maintenance, and the structure of this porous effectively can increase the transmission route of hertzian wave in wave absorbing agent inside, increase the effect of hertzian wave and wave absorbing agent, to electromagnetic absorption well, there is certain promoter action to realization.
Fig. 4 gives the statistics of the hole diameter size of the class worm hole porous carbon/magnetic particle composite wave-absorbing agent of preparation in embodiment 2, and known from statistic data, the size distribution of worm hole is between 40 ~ 100nm, and the proportion of 70nm is maximum.
Fig. 5 gives the energy spectrum analysis data of class worm hole porous carbon/magnetic particle composite wave-absorbing agent prepared by embodiment 2, and known, in the composite wave-absorbing agent of preparation, the content of carbon is 79.2%, and magnetic component content is 20.8%.
Fig. 6 gives the data of the reflection loss RL that the electromagnetic parameters that utilizes embodiment 3 to test to obtain obtains.As we know from the figure, material shows stronger electromaganic wave absorbing property.When thickness is 1.5mm, material shows hertzian wave K
uwave band absorbs preferably, and RL reaches 4GHz lower than the frequency span of-10dB.Continue the thickness increasing wave absorbing agent, absorption peak is moved to hertzian wave low frequency direction, still keeps the characteristic that wideband absorbs.When the thickness of wave absorbing agent reaches 4.0mm, material shows the characteristic of biabsorption frequency band, can simultaneously to electromagnetic C-band and K
ufrequency-range table reveals stronger absorption.Therefore, the material of preparation has wideband, thin matching thickness, the strong characteristic absorbed concurrently, shows electromagnetic C-band, X-band and K
uthe stronger receptivity of wave band.
Embodiment
Embodiment 1:
The synthetic method of the cobalt doped Fe 3 O 4 magnetic particle of coated with silica provided by the invention, realizes by following reactions steps:
(1) under nitrogen protection, in 200mL distilled water, 5.4mmol ferric chloride hexahydrate, 2.16mmol Iron dichloride tetrahydrate and 0.54mmol cobalt chloride hexahydrate is added, warming-in-water to 70 DEG C;
(2) adding strong aqua (mass percent 25 ~ 28%) is wherein 10 to pH, and continue reaction 60min, product Magneto separate reclaims, and uses distilled water and dehydrated alcohol respectively to wash 6 times recovery product, is scattered in 10mL distilled water;
(3) dispersion liquid is joined in 300mL ethanol, at 40 DEG C, add 6mL distilled water, 8mL strong aqua (mass percent 25 ~ 28%), 1.0mL tetraethyl orthosilicate, reaction 10h; Product uses Magneto separate, uses distilled water and dehydrated alcohol respectively to wash 6 times, is then placed in vacuum drying oven 70 DEG C of dry 12h, obtains the cobalt doped Z 250 particle of coated with silica.
Embodiment 2:
The synthetic method of class worm hole porous carbon/magnetic particle composite wave-absorbing agent provided by the invention, realizes by following reactions steps:
(1) the cobalt doped Z 250 particle of 0.32g coated with silica uses 14mL dimethyl formamide (DMF) ultrasonic disperse 2h, adds 2.4g polyacrylonitrile, 0.16g Polyvinylpyrolidone (PVP), 60 DEG C of heating for dissolving 2h;
(2) be poured on sheet glass by solution, use blade applicator knifing, proceeded in the container filling a large amount of distilled water, soak 24h, air drying 24h after taking out, obtains polyacrylonitrile/magnetic particle porous composite film;
(3) polyacrylonitrile of preparation/magnetic particle porous composite film is transferred in high temperature oven, 250 DEG C of heat treated 4h;
(4) by process after film transfer in high temperature process furnances, 1000 DEG C of vacuum carburization process 1h, obtain porous carbon/magnetic particle composite membrane, are fully ground by composite membrane, obtain class worm hole porous carbon/magnetic particle composite wave-absorbing agent.
Embodiment 3:
As the application of greying multi-walled carbon nano-tubes/Nanocomposites wave absorbing agent prepared by the present invention, be matrix with paraffin, prepared the test sample of different wave absorbing agent loading level, realized by following steps:
(1) paraffin and class worm hole porous carbon/magnetic particle composite wave-absorbing agent are mixed according to certain mass ratio; The mass percent of wherein wave absorbing agent/(wave absorbing agent+paraffin) is 30%;
(2) by the wave absorbing agent of upper step and the mixture of paraffin by mould use oil press to be suppressed into external diameter is 7mm, internal diameter is 3mm, thickness is 2mm test annulus;
(3) use Agilent N5244A PNA-X test the electromagnetic parameter of above-mentioned obtained sample within the scope of 2 ~ 18GHz (ε ', ε ", μ ', μ "), utilize the reflection loss RL of this composite wave-absorbing agent of formulae discovery.
Claims (6)
1. the preparation method of a kind worm hole porous carbon/magnetic particle composite wave-absorbing agent, its step is as follows:
(1) under nitrogen protection, to in 150 ~ 250mL distilled water, add 5 ~ 6mmol ferric chloride hexahydrate, 2.0 ~ 2.5mmol Iron dichloride tetrahydrate and 0.4 ~ 0.6mmol cobalt chloride hexahydrate, it is 9 ~ 11 that warming-in-water to 60 ~ 80 DEG C add strong aqua wherein to pH, continue reaction 30 ~ 90min, Magneto separate reclaims, and uses distilled water and dehydrated alcohol respectively to wash 5 ~ 8 times recovery product, is scattered in 5 ~ 15mL distilled water; Dispersion liquid is joined in 200 ~ 400mL ethanol, at 30 ~ 50 DEG C, add 5 ~ 7mL distilled water, 7 ~ 9mL strong aqua, 0.8 ~ 1.2mL tetraethyl orthosilicate, reaction 9 ~ 11h; Magneto separate reclaims, and uses distilled water and dehydrated alcohol respectively to wash 5 ~ 8 times recovery product, is then placed in vacuum drying oven 60 ~ 90 DEG C of drying 10 ~ 15h, obtains the cobalt doped Z 250 particle of coated with silica;
(2) the cobalt doped Z 250 particle of 0.25 ~ 0.40g coated with silica is used 12 ~ 16mL dimethyl formamide or N,N-DIMETHYLACETAMIDE, ultrasonic disperse 1 ~ 3h, add 2.0 ~ 3.0g polyacrylonitrile, 0.1 ~ 0.2g Polyvinylpyrolidone (PVP), 50 ~ 70 DEG C of heating for dissolving 1 ~ 3h, are poured into solution on the flat board of surfacing, soak 12 ~ 36h after knifing in distilled water, air drying 12 ~ 36h after taking out, obtains polyacrylonitrile/magnetic particle porous composite film;
(3) by polyacrylonitrile/magnetic particle porous composite film heat treated 3 ~ 6h at 200 ~ 300 DEG C of preparation, and then under 900 ~ 1100 DEG C of vacuum carbonizing treatment 0.5 ~ 2h, obtain porous carbon/magnetic particle composite membrane, composite membrane is fully ground, obtains class worm hole porous carbon/magnetic particle composite wave-absorbing agent.
2. a kind worm hole porous carbon/magnetic particle composite wave-absorbing agent, is characterized in that: be prepared by method according to claim 1.
3. a kind worm hole porous carbon/magnetic particle composite wave-absorbing agent as claimed in claim 2, is characterized in that: the ratio of porous carbon and magnetic particle is 75 ~ 85:15 ~ 25.
4. a kind worm hole porous carbon/magnetic particle composite wave-absorbing agent as claimed in claim 2, is characterized in that: the size of worm hole diameter is 40 ~ 100nm.
5. a kind worm hole porous carbon/magnetic particle composite wave-absorbing agent as claimed in claim 2, is characterized in that: be the absorbing material that matrix prepares different composite wave absorbing agent loading level further with paraffin.
6. a kind worm hole porous carbon/magnetic particle composite wave-absorbing agent as claimed in claim 5, it is characterized in that: be paraffin and class worm hole porous carbon/magnetic particle composite wave-absorbing agent are fully mixed, the mass percentage of wherein composite wave-absorbing agent is 25% ~ 35%.
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Cited By (3)
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| CN106495680A (en) * | 2016-11-08 | 2017-03-15 | 太原科技大学 | Carried magnetic metal simple-substance sheet calcium hexaluminate microwave absorbing ceramic compound material preparation method |
| CN106520071A (en) * | 2016-12-06 | 2017-03-22 | 吉林大学 | Rice husk based C/magnetic Co particle composite wave absorber and preparation method thereof |
| CN107835625A (en) * | 2017-09-18 | 2018-03-23 | 浙江理工大学 | Porous flake cobalt/carbon composite wave-suction material and preparation method thereof |
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| CN102134470A (en) * | 2010-10-20 | 2011-07-27 | 沈阳理工大学 | Method for preparing porous carbon born nano ferrite wave-absorbing material |
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| CN106495680A (en) * | 2016-11-08 | 2017-03-15 | 太原科技大学 | Carried magnetic metal simple-substance sheet calcium hexaluminate microwave absorbing ceramic compound material preparation method |
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| CN107835625A (en) * | 2017-09-18 | 2018-03-23 | 浙江理工大学 | Porous flake cobalt/carbon composite wave-suction material and preparation method thereof |
| CN107835625B (en) * | 2017-09-18 | 2020-06-02 | 浙江理工大学 | Porous sheet cobalt/carbon composite wave-absorbing material and preparation method thereof |
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